Process of distillation



Nov. 24, 1925.A l D. PYzl-:L

PROCESS OF DISTILLATION Original Filed Nov. 3. 1919 /NVEhF/)TOR DAN/EL VZEL 6v www ATTORNEYS Patented Nov; 24,: 1925.

' UNITED STATES PAT-E,

NT I OFFICE.

DANIEL PYzEL, or PIEDMCNT, CALIFORNIA, AssIGNoR, To SIMPLEX REFINING Colvi- PANY, oF SAN FRANCISCO, CALIFoa rnocnss orf NIA, A coaroaATIoN, or CALIFORNIA. l

DIsTILLATIoN.

.Application led November 3, 1919, 'Serial No. 335,537. i Renewed May-11, 1925.A

To all wlwm it may concern:

Be it known' that I, 'DANIEL FUEL, A'a

subject of the Queen of Holland, residing at Piedmont, in the county of Alameda and State' of California, have invented' .a new V and useful Improvement in the Art of -Distilling Bituminous Materials Comprising the Process of Distillation, of which the following is a specification. 'i

My invention relates to the art of distilling bituminous materials. It is particularly applicable 'to the distillation `of iasphaltum's, asphaltic residuums `and heavy petroleum oils, which although liquid at ordinary or higher temperatures', yield a f solid orsemisolid residuum in4 the process of distilling.

y the heavy asphaltic residuums of certain crude 'oils `and similar materials', is one which many refiners have been unable to meet. Althoughsuch residuums'have a limited'commercial The problem of disposing of Value in certain markets, there "is, in many places, an oversupply of such materials, which reduces their commercial value to an extremely low figure or even to such an extentthat they -canonly be considered as troublesome waste-products.. The transportation of. such materials to the markets by4 pipelines or tank-Steamers isimpossible .as they are only liquid athigh "temperatures, While atthe same time they are not sufficiently solid at ordinary temperatures to be transported in bulk 'as coal or 'coke is transported,l the-'pieces of thesematerials welding thelnselves together to a semi-solid mass when allowed to stand, this mass being extremely ditficultand costly to handle.`

Bituminous materials of a semi-solid nature can be vreduced to'products of a hi her tot-al commercial value by subjecting t em to a distillation 'to'dryness the products in this case being an oil distillate (fueloil) coke and gas. tillation process freheated stills or retorts of the usual types are used, the coke which is formedduring the process, settles on the Y' heatedbottoms and Walls of ysuch stills or 1'etorts,and prevents a ready transmission of the heat required for the distilling process. TheV rate 'of distillation and in ,co11- sequence the distilling capacity of the apparatus is thereby greatly reduced, other results being high fuel consumption,` over- However, if for such a disheating, blistering and rapid destruction of ithe still or retort material, and an excessive in most cases As regards 'the distillation 'of solid bituminous materials,

in the usual processes for distilling such materials, these substances are charged in externally fired retorts of various shapes,

inl which they are heate to a temperature sufficiently high to volatilize the bituminous matter and to form.

oily distillates and gases which in many cases contain considerable quantities of ammonia. -A very high temperature .is necesf sary to obtain `the largest possible yield of ammoniaJ while for the production of thev .maximum yield of valuable oily distillates a considerably lower temperature should not be exceeded.

'The slow rate of penetration ofthe `heat supplied to the retort Walls into the solid mass of the retort charge causes a very uueven distribution of this heat through the material in course of distillation, the result being that part of the oil vapors generated in the more centrally located and therefore cooler parts of the charge, are decomposed by contact with the overheated parts of the charge lying closer to the heated retort walls. g proposed to avoid this drawback, includingthe injection. of steam at the retort bottomto carry the oil vapors rapidly away and out of reach of the overheated, zone, and the use of stirring devices in the retorts, ,but all these methods are more orv Various methods have been y distilling bituminous materials in retorts I are the high fuel :consumption and the comparatively small distilling capacity of such retorts dueto thel slow traalmsmission of the required heat into the solid massof the retort charge. 1

An object of my invention is to provide mercially valuable oils, gas, and coke, coky substance or other solid matter.

vFurther objects and advantages will be made evident hereinafter.

For convenience, I have in the following description included heavy crude oils, asphaltic iesiduums, asphaltums and similar liquid or semi-solid materials under one general term as liquid bituminous material while mixtures of liquid bituminous material with extraneous matter are hereinafter calledv bituminous mixtures.

In the drawinfr which is extremely diagrammatic and in which no attempt has been made to preserve the proper proportion of the parts, 1 is a rotary kiln,2 isa condenser, 3 is a gas separator or trap, 4 is a scrubber, 5 is a cold gas blower, 6 is a hot gas inlet, 7 is-a bin, 8 is a crushing and mixing apparatus, and 9 is a feeder. p

Each of these pieces of apparatusgis well known in the arts and various types thereof can be employed without departing from the spirit of my invention or exercising more thanmere mechanical skill, thety es shown being merely selected as of a class.

The rotary .kiln 1 is similar in construction to the st'andard type of kiln used for manufacturing Portland cement except that it is provided with 'a somewhat better closure means at either end for the purpose .of reillustrative taining the gases therein.

Liquid bituminous material is delivered to the crushing and mixing apparatus 8 where it can be mixed with solid or liquid extraneous substances to a bituminous mixtiu'e which is delivered from the mixerby means of the feeder 9 into the upper end of the rotary kiln 1.

This bituminous mixture must be of such a consistency `that during its passage through the rotating lkiln 1, where it is subjected to the action of hot gases, it will at no time stick or adhere to the walls of this kiln, but will formlumpsor' marbles of a suitable size to allow a rapid penetration of the heat therein while the combined action of the rotation and the inclination of the kiln causes these lumps on marbles to be gradually moved to the lower end ofl the kiln.

For the purpose of producing a material having the characteristics I mix liquid bituminous materials with extraneous qsolids like sand, sawdust, powdered Icoke, powdered coal, oil sand or other material, to form a coherent but non-adherent pasty mixture, the percentage of adinixture being largely dependent on the character of the bituminous mattei' to be treated.

During the passage of the bituminous mixture through the kiln which is rotated by any convenient means (not shown) it is subjected to the action ofhot gases, these gases servi-ng to thoroughlyheat the pieces, lumps or marbles of bituminous mixture, and drive off all the volatile constituents thereof. As the mixture slowly moves inV counter current to the hot gases, and the smallsize of the lumps of material allows a rapid penetration of the heat therein, this volatile matter is carried off at comparativel low temperatures, especially as the large volume of the heating gases causes the oil constituents to evaporate at temperatures below their normal boiling points. Moreover, these volatile `matters are immediately carriedoff to coolei Zones of the kiln so that the danger of the oil vapors being decomposed by yexcessively high temperatures is greatly diminished.

The non-volatile solid residuuni of the bituminous mixture left after driving off its volatile constituents is delivered from thel lower or discharge end of the kiln intolthe bin, 7. According to the character of the bituminous material charged and of the mixture, this residuum may be a commeicially valuable product like coke, or a less valuable mixture of coke and mineral mattei'` or even a valueless mineral matter like spent shale. This solid residuuin is discharged from the bin and disposed of in a .suitable way, and in case a liquid bituminous material is treated, which requires an admixtui'e .of solid matter to give itthe proper consistency for the process, part `of this solid residuiiin may be returned to the mixing apparatus 8.

The volatile products driven off from the bituminous mixture by the action of the hot gases are carried together with these gases from the upper end of the rotary kiln through the pipe 10, to the condenser oi cooler 2. This apparatus may be iii the form of a tubular watercooled condenser as shown in the diagram, or it may be in the 'form of any other cooling or condensing apparatus known in the arts and suitable for the purpose,I like air-cooled or watersprayed coolers. In this cooler or. condenser the mixture of gases and vapors is reduced to a low temperature, so that the majority of the vapors are condensed and precipitated. The condensate which consists mainly of oil distillates but which may also contain other liquids, like ammoniacal water and other watery solutions, dependent on the character of the bituminous material treated, is separated from the remaining un- CII weaves.

condensed gases by means of the gas separa-tor or trap 3, and carried oit' to a suitable receiver through the pipe 12.

The remaining gasesrwhich may still contain vapors of desirable products, are then passed through the pipe`13, to the scrubber Ll, where they are further freed from such products. The form of scrubber to be used is also dependent on the character of 4the crude material treated and the products to be collected. rlhe diagram shows one scrubber only, but a plurality of apparatus ot various wellknown forms may be used to i'rce the gases ofliquid oil carried over in the shape ot a fog or mist, and ot vapors of light hydrocarbons and other substances like ammonia gas. Such products are carried olf together with the absorbing medium used in the scrubbing process through the pipe 14, to a suitable receiver.

The permanent gases leave the scrubbing apparatus through the pipe 15, and can be carried away through the outlet 16, t0 be used foi-.any purpose for which they are suitable. yPart of these frases can also be led through the pipe 17pto the cold gas blower 5, which delivers the gas to the lower or heating end of the rotary kiln 1.

It is of the utmost importance 4in order to obtain the highest possible output of valuable products trom the bituminous material treated, to provide means for the exact adtion gases obtained in this Way will haveV a temperature far'in excess of the maximum which can be allowed at the point Where these, gases enter the kiln, and their ternperat'ure must therefore be reduced to this maximum. It is obvious that this can be done byusing the excess heat of these gases iorjother purposes before they are introduced to the kiln. tatesthe combination of the rotary kiln with other apparatus which in many cases will be'yyiiounzl to be impracticable. n such cases l 'reduce the temperatureof the hot combustion gases either by injecting steam or a finely divided spray of water into these gases before they enter the kiln, for which purpose the steam or water spray-apparatus 1S is connected to the hot-gas inlet 6, or by mixingthem with cold gas, drawn by the blower 5 through the Apipe 17 from the scrubber outlet 15.

By vusing any ot' these three methods alone or in combination, the temperature of the gas entering the kiln can be accurately adjusted so as to obtain the highest possible yield of valuable products.

I claim as my invention l This, however, necessil. A process ot reining liquid bituminous material which comprises: mixing said material with solid matter to form a bituminous mixture; rolling said bituminous mixture in the form of coherent balls through a chamber, and passing hot non-oxidizing gases through said chamber in contact with `said balls.

2. A process of refining liquid bituminous material which comprises: mixing said material with solid matter to form a bituminous mixture; rolling said bituminous mixture in the form ot' coherent balls through a rotating chamber; and passing hot nonoxidizing gases through said chamber in contact `with said balls.

In testimony whereof, I have hereunto set my hand atSan Francisco, alifornia, tl .is 22nd day of* October, 1919;.

DANIEL PY'ZEL.y 

